Recently, chemical vapor deposition has been used in the manufacturing procedures for thin copper membranes. For example, CVD is used for the manufacturing of thin membranes for superconductors, copper wiring for various ICs, and compound semiconductors (called chalcopyrite) such as Cu.sub.x In.sub.y (Al, CA) S.sub.n (Se).
The material for this CVD is, for example the .beta. Copper diketone complex shown in Exhibit 1. ##STR1## [R is a methyl radical, t is a butyl radical or a trifluoromethyl radical. ]
This compound is not suitable for CVD, where a sublimation transportation is used. This compound is solid; thus, it is not suitable for a mass transportation. It is also not suitable for industrial production due to its high disintegration temperature and the slow speed at which it forms thin copper membranes.
To solve this problem, a .beta. copper diketone complex consisting HfaCu(I).L is developed as shown in Exhibit 2. ##STR2## [L is an additional cuprous, an electronic donator.]
The compound shown in Exhibit 2 is suitable for CVD because its fusing point is below 100.degree. C., L is liquid when it is TMVS, and the compound's steam pressure is higher than the one for the compound shown in Exhibit 1.
The following method 1 is known as composite procedures:
(1) Cu.sub.2 O+2Hfa(H)+2L .fwdarw.2HfaCu.L+H.sub.2 O [Hfa (H)=1,1,1,5,5,5-Hexaflouoro-2, 4-pentanedione] PA1 (2) CuX+HfaM+L .fwdarw.HfaCu.L+MX [X is a halogen atom, M is alkali metal such as Li, Na, K.]
Currently, this method is not used for industrial production because HfaCu.L disintegrates in a short time.
This method 2 does not have the problem of the method (1), the HfaCu.L disintegrates in a short time. However, it has a contamination problem with halogen atoms and alkali metals. A distillate purification is performed to remove these impurities; however, the yield is reduced significantly due to the instability of HfaCu.L.
Also, the separation of HfaCu.L and the crude materials, such as HfaNa, are difficult due to the materials' steam pressure. This makes it difficult to acquire high-purity HfaCu.L. Moreover, the materials, such as CuX and HfaM are expensive; thus, method (2) costs 10 times more than method (1).
An object of the subject invention is to provide a high-purity copper complex (a .beta. copper diketone complex) such as HfaCu(I).L, shown in Exhibit 2, at a low cost.
This invention regards the manufacturing procedures of a .beta. copper diketone complex which consist of: the first process, mixing and reacting Cu.sub.2 O, 1, 1, 1, 5, 5, 5-Hexafluoro-2, 4-pentanedione and an additional cuprous L, an electronic donator; and the second process, dehydrating the crude material such as by using a dehydrating agent, which is performed at the same time and/or right after the reaction in the first process.
This invention also regards the manufacturing procedures of a .beta. copper diketone complex which consist of: the third process, the purification of the crude material via a column chromatogram (for example, a column chromatogram filled with silica gel and/or alumina) .